CN109970458A - A kind of modified carbonaceous chute and preparation method thereof - Google Patents
A kind of modified carbonaceous chute and preparation method thereof Download PDFInfo
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
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Abstract
The invention discloses a kind of modified carbonaceous chutes and preparation method thereof.The carbonaceous chute includes castable and the graphite material as aggregate, and the weight ratio of graphite material and castable is 1:(3~7), wherein graphite material includes following raw material components by weight: 25~40 parts of graphite；30~55 parts of needle coke；15~25 parts of pitch.Carbonaceous chute of the invention can reduce the oxidation rate of carbonaceous chute, and tolerance high temperature is come out of the stove the erosion of material, service life be significantly increased, while having very high mechanical strength and flexural strength, it is not easy to crack, fracture occur.
Description
Technical field
The present invention relates to a kind of modified carbonaceous chute and preparation method thereof, in particular to a kind of high temperature resistant, good toughness change
Property carbonaceous chute preparation method.
Background technique
Mineral hot furnace is also known as electric-arc furnace or resistance electric furnace, mainly for the production of products such as industrial silicon, calcium carbide, yellow phosphorus, at this
Industry is also commonly called as electric furnace.
Construction is mainly made of carbon brick, furnace eye and channel of coming out of the stove in furnace shell, furnace in furnace.For example, when production metallic silicon,
With the silica in carbonaceous reducing agent silica in Lu Nei crucible area, the metallic silicon (up to 1500 DEG C) of molten state is generated,
Then it is flowed into silicon packet by the chute of furnace eye.Since furnace eye is continuously come out of the stove, existing carbonaceous chute oxidation rate is fast, and carbonaceous is slipped
Slot is easily burnt, and causes blowing out repeatedly or scaling loss equipment, seriously affects the normal production of electric furnace.Furthermore the metallic silicon stream of molten state
The problems such as when crossing carbonaceous chute, temperature is steeply risen, and is easy to appear crack, fracture.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of modified carbonaceous chutes and preparation method thereof.Of the invention
Modified carbonaceous chute can reduce the oxidation rate of carbonaceous chute, and tolerance high temperature is come out of the stove the erosion of material, and being significantly increased makes
With the service life, while there is very high mechanical strength and flexural strength, it is not easy to crack and fracture occur.
The present invention provides a kind of modified carbonaceous chutes comprising castable and the graphite material as aggregate, graphite material
Material and the weight ratio of castable are 1:(3~7), wherein graphite material includes following raw material components by weight:
25~40 parts of graphite powder；
30~55 parts of needle coke；
15~25 parts of pitch.
Further, the pitch uses coal tar pitch, and softening point is 70~90 DEG C, and preferably coal tar pitch is paraformaldehyde and first
The coal tar pitch of sulfonic acid modified.
Further, in modified coal pitch, coal tar pitch and paraformaldehyde, methanesulfonic acid weight ratio be 10:(0.5~
3.5): (0.05~0.5).
Further, the degree of polymerization of paraformaldehyde is 8~100, preferably 10~50.
Further, the density of needle coke is 2.0~2.3g/cm3, ash content≤1.1%, length-width ratio is 1.6~2.0.
Further, the weight content of castable component are as follows: Al2O3≥86%、Fe2O3≤1.5%、Ti2O3≤ 3.0%, preferably
Are as follows: 96%~99.5%Al2O3, 0.1%~1.5%Fe2O3, 0.3%~3.0%Ti2O3。
Further, graphite material is cylindrical and/or cuboid.
The present invention also provides a kind of preparation methods such as above-mentioned modification carbonaceous chute comprising following steps:
(1) kneading machine being added in graphite powder, needle coke and carries out dry-mixed, dry-mixed temperature is 120~170 DEG C, the time is 20~
90min adds pitch and carries out wet mixing after mixing, and the temperature of wet mixing is 120~170 DEG C, and the time is 25~90min,
Wet mixing is placed on extrusion forming in extruder, obtains blank；
(2) blank obtained by step (1) is placed in roaster and is roasted, obtain roasting product, the temperature of roasting is 900~1200
DEG C, the time is 24~120 h；
(3) roasting product obtained by step (2) is placed in graphitizing furnace and is graphitized, graphited temperature is 2600~3100
DEG C, the time is 12~120 h, obtains graphite material；
(4) water, weight ratio 100:(0.5~10 of castable and water are added in castable), after mixing, obtain wet
Material；
(5) graphite material is placed in mold, and step (4) resulting wet feed is then added, forms after casting, carries out after the drying
Demoulding, then roasts 5~15 days at 500~600 DEG C, obtains modified carbonaceous chute.
Further, it further includes changing to pitch preferably before kneading machine is added in pitch that the pitch, which is coal tar pitch,
Property the step of: in coal tar pitch be added paraformaldehyde aqueous solution, methanesulfonic acid, be heated to 95~120 DEG C of 0.5~4h of reaction, obtain
To modified coal tar pitch.
Further, in step (1), the pressure of extrusion forming is 5~15MPa；In step (5), dry temperature
It is 40~110 DEG C, the time is 5~120 h.
Compared with prior art, modification carbonaceous chute and preparation method thereof of the invention has the advantages that
(1) modification carbonaceous chute of the invention, including castable and as the graphite material of aggregate, especially graphite material is with stone
Ink powder, needle coke, pitch are raw material, and further the pitch coal tar pitch modified using paraformaldehyde, methanesulfonic acid, is then infused with burning
Material is used cooperatively, and can reduce the oxidation rate of carbonaceous chute, and tolerance high temperature is come out of the stove the erosion of material, has been significantly increased and has been come out of the stove
Frequency of usage reaches 160 times.
(2) carbonaceous chute of the invention has very high mechanical strength and flexural strength, so as to bear high temperature
Impact when furnace charge is come out of the stove, it is not easy to crack and fracture occur.
(3) density of needle coke of the invention is 2.0~2.3g/cm3, ash content≤1.1%, length-width ratio is 1.6~2.0,
The needle coke of such aspect ratio is conducive to further increase erosion resistance, prevents the appearance of crack and fracture.
(4) weight content of castable component of the invention are as follows: Al2O3≥86%、Fe2O3≤1.5%、Ti2O3≤ 3.0%, this
Sample helps to improve erosion resistance, prevents the appearance of crack and fracture.
Specific embodiment
The technical solution that the invention is further illustrated by the following examples, but these embodiments cannot limit it is of the invention
Protection scope.
Embodiment 1
(1) aqueous solution, the methanesulfonic acid of paraformaldehyde (degree of polymerization 40) are added in coal tar pitch (softening point is 80 DEG C), is heated to
110 DEG C of reaction 2h, obtain modified coal tar pitch.The weight ratio of coal tar pitch and paraformaldehyde, methanesulfonic acid is 10:2.5:0.1.
(2) by 30 parts by weight of graphite powder, 40 parts by weight needle cokes, (density of needle coke is 2.1g/cm first3, ash content≤
1.0%, length-width ratio 1.8) kneading machine is added to carry out dry-mixed, dry-mixed temperature is 150 DEG C, time 60min, it is uniformly mixed
Afterwards, 20 part by weight modified coal tar pitch are added and carry out wet mixing, the temperature of wet mixing is 150 DEG C, time 50min, in wet mixing postposition
The pressure of the extrusion forming in extruder, extrusion forming is 10MPa, obtains cylindrical blank, the diameter 80mm of blank, length
80mm；
(3) blank obtained by step (2) being placed in roaster and is roasted, obtain roasting product, the temperature of roasting is 1000 DEG C, when
Between be 30 h；
(4) roasting product obtained by step (3) is placed in graphitizing furnace and is graphitized, graphited temperature is 3000 DEG C, the time
For 40 h, graphite material is obtained；
(5) in castable (97%Al2O3、1.0%Fe2O3、2.0%Ti2O3) in addition water obtain wet feed after mixing, be poured
The weight ratio 100:2 of material and water；
(6) mold is made with the iron plate of long 800mm wide 400mm high 400mm, the good rear surface of Mold Making applies one layer of used oil, just
In demoulding；Graphite material is discharged in mold, and step (5) resulting wet feed is then added, forms after casting, carries out after the drying
Demoulding, dry temperature are 50 DEG C, and the time is 80 h, is then roasted 10 days at 550 DEG C, obtain modified carbonaceous chute.Wherein,
Graphite material and the weight ratio of castable are 1:5.
Embodiment 2
(1) aqueous solution, the methanesulfonic acid of paraformaldehyde (degree of polymerization 40) are added in coal tar pitch (softening point is 85 DEG C), is heated to
120 DEG C of reaction 1.5h, obtain modified coal pitch.The weight ratio of coal tar pitch and paraformaldehyde, methanesulfonic acid is 10.0:3.0:
0.08。
(2) by 35 parts by weight of graphite powder, 45 parts by weight needle cokes, (density of needle coke is 2.1g/cm first3, ash content≤
1.0%, length-width ratio 1.8) kneading machine is added to carry out dry-mixed, dry-mixed temperature is 140 DEG C, time 60min, it is uniformly mixed
Afterwards, 25 part by weight modified coal tar pitch are added and carry out wet mixing, the temperature of wet mixing is 140 DEG C, time 50min, in wet mixing postposition
The pressure of the extrusion forming in extruder, extrusion forming is 10MPa, obtains cylindrical blank, the diameter 80mm of blank, length
80mm；
(3) blank obtained by step (2) being placed in roaster and is roasted, obtain roasting product, the temperature of roasting is 1100 DEG C, when
Between be 30 h；
(4) roasting product obtained by step (3) is placed in graphitizing furnace and is graphitized, graphited temperature is 3100 DEG C, the time
For 35 h, graphite material is obtained；
(5) in castable (96.1%Al2O3、1.2%Fe2O3、2.7%Ti2O3) in addition water obtain wet feed after mixing, pour
The weight ratio 100:2.5 of material feeding and water；
(6) mold is made with the iron plate of long 800mm wide 400mm high 400mm, the good rear surface of Mold Making applies one layer of used oil, just
In demoulding；Graphite material is discharged in mold, and step (5) resulting wet feed is then added, forms after casting, carries out after the drying
Demoulding, dry temperature are 50 DEG C, and the time is 80 h, is then roasted 10 days at 550 DEG C, obtain modified carbonaceous chute.Wherein,
Graphite material and the weight ratio of castable are 1:6.
Embodiment 3
(1) aqueous solution, the methanesulfonic acid of paraformaldehyde (degree of polymerization 40) are added in coal tar pitch (softening point is 80 DEG C), is heated to
110 DEG C of reaction 2h, obtain modified coal pitch；The weight ratio of coal tar pitch and paraformaldehyde, methanesulfonic acid is 10.0:3.0:0.07.
(2) by 35 parts by weight of graphite powder, 50 parts by weight needle cokes, (density of needle coke is 2.1g/cm first3, ash content≤
1.0%, length-width ratio 1.8) kneading machine is added to carry out dry-mixed, dry-mixed temperature is 145 DEG C, time 60min, it is uniformly mixed
Afterwards, 23 part by weight modified coal tar pitch are added and carry out wet mixing, the temperature of wet mixing is 155 DEG C, time 50min, in wet mixing postposition
The pressure of the extrusion forming in extruder, extrusion forming is 10Mpa, obtains cylindrical blank, the diameter 80mm of blank, length
80mm；
(3) blank obtained by step (2) being placed in roaster and is roasted, obtain roasting product, the temperature of roasting is 1000 DEG C, when
Between be 30 h；
(4) roasting product obtained by step (3) is placed in graphitizing furnace and is graphitized, graphited temperature is 2900 DEG C, the time
For 60 h, graphite material is obtained；
(5) in castable (96.3%Al2O3、1.2%Fe2O3、2.5%Ti2O3) in addition water obtain wet feed after mixing, pour
The weight ratio 100:8 of material feeding and water；
(6) mold is made with the iron plate of long 800mm wide 400mm high 400mm, the good rear surface of Mold Making applies one layer of used oil, just
In demoulding；Graphite material is discharged in mold, and step (5) resulting wet feed is then added, forms after casting, carries out after the drying
Demoulding, dry temperature are 50 DEG C, and the time is 80 h, is then roasted 10 days at 550 DEG C, obtain modified carbonaceous chute.Wherein,
Graphite material and the weight ratio of castable are 1:4.
Embodiment 4
The preparation method of the present embodiment is substantially same as Example 1, and difference is: the step of saving embodiment 1 (1), coal drip
Blueness directlys adopt the coal tar pitch raw material not being modified in wet mixing step without modification procedure.
Comparative example 1
This comparative example is substantially the same manner as Example 1, and difference is using commercially available cylindric graphite (Yixing City rising sun graphite system forever
Product Co., Ltd, model: yx-2) alternate embodiment 1 graphite material.
Comparative example 2
The chute of this comparative example is made of pouring material, does not add graphite material.
(1) in castable (97%Al2O3、1.0%Fe2O3、2.0%Ti2O3) in addition water obtain wet feed after mixing,
The weight ratio 100:2 of castable and water；
(2) mold is made with the iron plate of long 800mm wide 400mm high 400mm, the good rear surface of Mold Making applies one layer of used oil, just
In demoulding；Then step (2) resulting wet feed is added, forms after casting, is demoulded after the drying, dry temperature is 50
DEG C, the time is 80 h, then roasts 10 days at 550 DEG C, obtains chute.
Test case 1
The carbonaceous chute the performance test results of embodiment 1-4 and comparative example 1 are shown in Table 1.
The carbonaceous chute the performance test results of 1 embodiment 1-4 of table and comparative example 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example 1 | |
| Compression strength, MPa | 68 | 72 | 70 | 60 | 51 |
| Bending strength, MPa | 31.4 | 32.6 | 33.5 | 28.4 | 20.4 |
| Shore hardness | 54 | 53 | 51 | 49 | 42 |
The modified carbonaceous chute of the present invention has very high mechanical strength and bending strength, so as to bear rushing for high-temp. furnace material
It hits, it is not easy to crack and fracture occur.
Test case 2
The chute of embodiment 1-4 and comparative example 1,2 are arranged in the furnace eye of industrial silicium mine hot stove, then carry out industrial silicon material
Production, the frequency of usage of chute are shown in Table 2.
The frequency of usage of 2 embodiment 1-4 of table and the chute of comparative example 1,2
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example 1 | Comparative example 2 | |
| Frequency of usage | 160 | 157 | 152 | 123 | 93 | 1 |
Since the carbonaceous chute oxidation rate of comparative example 1 is fast, furnace charge corrodes seriously carbonaceous chute, causes the service life shorter；Comparison
The chute of example 2 carries out industrial silicon production, and when first used, breakage problem just occurs in most of chute, cannot be by the gold of molten state
Belong to silicon and is successfully discharged into silicon packet；And the modified carbonaceous chute of the present invention can high temperature resistant, anti-oxidant and anti-erosion is strong, and frequency of usage reaches
160 heats.
Claims (10)
1. a kind of modified carbonaceous chute, which is characterized in that it includes castable and the graphite material as aggregate, graphite material with
The weight ratio of castable is 1:(3~7), wherein graphite material includes following raw material components by weight:
25~40 parts of graphite powder；
30~55 parts of needle coke；
15~25 parts of pitch.
2. carbonaceous chute according to claim 1, which is characterized in that the pitch use coal tar pitch, softening point be 70~
90 DEG C, preferably coal tar pitch is the coal tar pitch that paraformaldehyde and methanesulfonic acid are modified.
3. carbonaceous chute according to claim 2, which is characterized in that in modified coal pitch, coal tar pitch and paraformaldehyde, first
The weight ratio of sulfonic acid is 10:(0.5~3.5): (0.05~0.5).
4. carbonaceous chute according to claim 2 or 3, which is characterized in that the degree of polymerization of paraformaldehyde is 8~100, preferably
It is 10~50.
5. carbonaceous chute according to claim 1 to 3, which is characterized in that the density of needle coke is 2.0~2.3g/
cm3, ash content≤1.1%, length-width ratio is 1.6~2.0.
6. carbonaceous chute according to claim 1 to 3, which is characterized in that the weight content of castable component are as follows:
Al2O3≥86%、Fe2O3≤1.5%、Ti2O3≤ 3.0%, preferably are as follows: 96%~99.5%Al2O3, 0.1%~1.5%Fe2O3, 0.3%~
3.0%Ti2O3。
7. carbonaceous chute according to claim 1 to 3, which is characterized in that graphite material is cylindrical and/or rectangular
The bodily form.
8. a kind of preparation method of modified carbonaceous chute as claimed in claim 1, which is characterized in that it includes as follows
Step:
(1) kneading machine being added in graphite powder, needle coke and carries out dry-mixed, dry-mixed temperature is 120~170 DEG C, the time is 20~
90min adds pitch and carries out wet mixing after mixing, and the temperature of wet mixing is 120~170 DEG C, and the time is 25~90min,
Wet mixing is placed on extrusion forming in extruder, obtains blank；
(2) blank obtained by step (1) is placed in roaster and is roasted, obtain roasting product, the temperature of roasting is 900~1200
DEG C, the time is 24~120 h；
(3) roasting product obtained by step (2) is placed in graphitizing furnace and is graphitized, graphited temperature is 2600~3100
DEG C, the time is 12~120 h, obtains graphite material；
(4) water, weight ratio 100:(0.5~10 of castable and water are added in castable), after mixing, obtain wet
Material；
(5) graphite material is placed in mold, and step (4) resulting wet feed is then added, forms after casting, carries out after the drying
Demoulding, then roasts 5~15 days at 500~600 DEG C, obtains modified carbonaceous chute.
9. preparation method according to claim 8, which is characterized in that the pitch is coal tar pitch, is preferably added in pitch
Before kneading machine, further include the steps that being modified pitch: aqueous solution, the methanesulfonic acid of paraformaldehyde being added in coal tar pitch,
95~120 DEG C of 0.5~4h of reaction are heated to, modified coal tar pitch is obtained.
10. preparation method according to claim 8 or claim 9, which is characterized in that in step (1), the pressure of extrusion forming is
5~15MPa；In step (5), dry temperature is 40~110 DEG C, and the time is 5~120 h.
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| CN110041086A (en) * | 2019-05-13 | 2019-07-23 | 中冶武汉冶金建筑研究院有限公司 | A kind of flexible carbonaceous castable for furnace bottom screed-coat |
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